#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308543.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308543
loop_
_publ_author_name
'Nancy L. S. Yue'
'Michael C. Jennings'
'Richard J. Puddephatt'
_publ_section_title
;
Disilver(I) Macrocycles: Variation of Cavity Size with Anion Binding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1125
_journal_page_last               1131
_journal_paper_doi               10.1021/ic048549c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C42.5 H41 Ag2 B2 Cl5 F8 N8 O4'
_chemical_formula_weight         1294.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9602(3)
_cell_length_b                   9.5276(2)
_cell_length_c                   17.7105(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2625.89(10)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'phi/omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25633
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.5195
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4623
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0786P)²+2.5556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                3479
_reflns_number_total             4623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048549csi20041015_044205_4.cif
_cod_data_source_block           2d
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2625.89(9)
_cod_original_formula_sum        'C42.50 H41 Ag2 B2 Cl5 F8 N8 O4'
_cod_database_code               4308543
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.50452(2) 2.70431(4) 1.62051(2) 0.03858(17) Uani 1 1 d . . .
N11 N 0.5876(2) 2.8086(4) 1.7295(2) 0.0335(9) Uani 1 1 d . . .
C12 C 0.6406(3) 2.7379(5) 1.7962(3) 0.0335(11) Uani 1 1 d . . .
H12A H 0.6408 2.6383 1.7942 0.040 Uiso 1 1 calc R . .
C13 C 0.6939(3) 2.8034(5) 1.8665(3) 0.0364(11) Uani 1 1 d . . .
H13A H 0.7304 2.7497 1.9123 0.044 Uiso 1 1 calc R . .
C14 C 0.6945(3) 2.9492(5) 1.8709(3) 0.0317(10) Uani 1 1 d . . .
C15 C 0.6389(3) 3.0215(5) 1.8031(3) 0.0337(11) Uani 1 1 d . . .
H15A H 0.6360 3.1210 1.8043 0.040 Uiso 1 1 calc R . .
C16 C 0.5879(3) 2.9491(5) 1.7342(3) 0.0338(11) Uani 1 1 d . . .
H16A H 0.5511 3.0007 1.6876 0.041 Uiso 1 1 calc R . .
N17 N 0.7497(3) 3.0183(4) 1.9435(2) 0.0377(10) Uani 1 1 d . . .
C18 C 0.7554(5) 2.9626(7) 2.0236(3) 0.072(2) Uani 1 1 d . . .
H18A H 0.7950 3.0207 2.0682 0.108 Uiso 1 1 calc R . .
H18B H 0.7766 2.8658 2.0302 0.108 Uiso 1 1 calc R . .
H18C H 0.6984 2.9644 2.0253 0.108 Uiso 1 1 calc R . .
C19 C 0.7905(3) 3.1426(5) 1.9446(3) 0.0314(10) Uani 1 1 d . . .
O20 O 0.8221(2) 3.2111(3) 2.0083(2) 0.0401(8) Uani 1 1 d . . .
N21 N 0.4179(2) 2.5996(4) 1.5138(2) 0.0331(9) Uani 1 1 d . . .
C22 C 0.3642(3) 2.5000(5) 1.5185(3) 0.0391(12) Uani 1 1 d . . .
H22A H 0.3677 2.4733 1.5714 0.047 Uiso 1 1 calc R . .
C23 C 0.3046(3) 2.4348(5) 1.4509(3) 0.0380(12) Uani 1 1 d . . .
H23A H 0.2671 2.3661 1.4573 0.046 Uiso 1 1 calc R . .
C24 C 0.2993(3) 2.4700(5) 1.3730(3) 0.0290(10) Uani 1 1 d . . .
C25 C 0.3561(3) 2.5692(5) 1.3675(3) 0.0304(10) Uani 1 1 d . . .
H25A H 0.3561 2.5940 1.3155 0.036 Uiso 1 1 calc R . .
C26 C 0.4130(3) 2.6318(5) 1.4384(3) 0.0336(11) Uani 1 1 d . . .
H26A H 0.4507 2.7016 1.4336 0.040 Uiso 1 1 calc R . .
N27 N 0.2404(2) 2.3992(4) 1.3035(2) 0.0326(9) Uani 1 1 d . . .
C28 C 0.2264(3) 2.2480(6) 1.3132(3) 0.0428(13) Uani 1 1 d . . .
H28A H 0.1840 2.2109 1.2613 0.064 Uiso 1 1 calc R . .
H28B H 0.2053 2.2357 1.3569 0.064 Uiso 1 1 calc R . .
H28C H 0.2808 2.1973 1.3278 0.064 Uiso 1 1 calc R . .
C29 C 0.1995(3) 2.4562(5) 1.2264(3) 0.0328(11) Uani 1 1 d . . .
O30 O 0.1635(2) 2.3813(4) 1.16662(19) 0.0411(8) Uani 1 1 d . . .
C31 C 0.8005(3) 3.1918(5) 1.8687(3) 0.0320(11) Uani 1 1 d . . .
C32 C 0.7928(3) 3.3338(5) 1.8519(3) 0.0304(10) Uani 1 1 d . . .
H32A H 0.7794 3.3956 1.8872 0.036 Uiso 1 1 calc R . .
C33 C 0.8044(3) 3.3878(5) 1.7842(3) 0.0325(11) Uani 1 1 d . . .
C34 C 0.8283(3) 3.2978(5) 1.7346(3) 0.0375(12) Uani 1 1 d . . .
H34A H 0.8364 3.3334 1.6881 0.045 Uiso 1 1 calc R . .
C35 C 0.8401(3) 3.1565(6) 1.7538(3) 0.0414(12) Uani 1 1 d . . .
H35A H 0.8582 3.0959 1.7212 0.050 Uiso 1 1 calc R . .
C36 C 0.8261(3) 3.1023(5) 1.8197(3) 0.0371(11) Uani 1 1 d . . .
H36A H 0.8337 3.0048 1.8318 0.044 Uiso 1 1 calc R . .
B40 B 0.5577(9) 2.9774(16) 1.5184(8) 0.067(5) Uani 0.50 1 d PD A -1
F41 F 0.4816(5) 2.9923(19) 1.5212(10) 0.143(6) Uani 0.50 1 d PD A -1
F42 F 0.5779(5) 2.8396(8) 1.5203(5) 0.084(3) Uani 0.50 1 d PD A -1
F43 F 0.6094(6) 3.0480(8) 1.5836(4) 0.083(2) Uani 0.50 1 d PD A -1
F44 F 0.5560(6) 3.0420(8) 1.4497(4) 0.068(2) Uani 0.50 1 d PD A -1
B50 B 0.4917(12) 3.3531(10) 1.7474(19) 0.032(3) Uani 0.50 1 d PD B -1
F51 F 0.5185(12) 3.267(3) 1.6982(12) 0.037(3) Uani 0.50 1 d PD B -1
F52 F 0.4057(4) 3.3884(7) 1.7075(4) 0.0476(15) Uani 0.50 1 d PD B -1
F53 F 0.5392(5) 3.4752(8) 1.7680(5) 0.073(2) Uani 0.50 1 d PD B -1
F54 F 0.5058(12) 3.283(3) 1.8210(13) 0.043(4) Uani 0.50 1 d PD B -1
C71 C 0.9874(8) 2.7294(14) 1.6749(9) 0.068(4) Uani 0.50 1 d PD C 1
H71A H 1.0331 2.7191 1.6538 0.082 Uiso 0.50 1 calc PR C 1
H71B H 0.9313 2.7173 1.6280 0.082 Uiso 0.50 1 calc PR C 1
Cl72 Cl 1.0000 2.5965(3) 1.7500 0.0709(6) Uani 1 2 d SD . 1
Cl73 Cl 0.9927(3) 2.8938(4) 1.7154(3) 0.101(2) Uani 0.50 1 d PD . 1
C81 C 0.9669(7) 2.6569(16) 2.0387(16) 0.113(9) Uani 0.50 1 d PD D 2
H81A H 0.9797 2.6029 1.9971 0.136 Uiso 0.50 1 calc PR D 2
H81B H 1.0169 2.6470 2.0919 0.136 Uiso 0.50 1 calc PR D 2
Cl82 Cl 0.8849(3) 2.5876(4) 2.0477(2) 0.0659(9) Uani 0.50 1 d PD D 2
Cl83 Cl 0.9562(3) 2.8386(7) 2.0096(4) 0.115(2) Uani 0.50 1 d PD D 2
C91 C 0.9734(16) 2.705(2) 2.0125(13) 0.029(5) Uiso 0.25 1 d PD E 3
H91A H 0.9492 2.6617 1.9572 0.035 Uiso 0.25 1 calc PR E 3
H91B H 1.0354 2.6814 2.0361 0.035 Uiso 0.25 1 calc PR E 3
Cl92 Cl 0.9331(10) 2.6179(15) 2.0663(8) 0.112(4) Uiso 0.25 1 d PD E 3
Cl93 Cl 0.9689(6) 2.8841(11) 1.9951(6) 0.073(3) Uiso 0.25 1 d PD . 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 Ag N11 177.73(14) . . ?
C16 N11 C12 117.4(4) . . ?
C16 N11 Ag 120.5(3) . . ?
C12 N11 Ag 122.1(3) . . ?
N11 C12 C13 122.8(4) . . ?
C12 C13 C14 119.6(4) . . ?
C15 C14 C13 117.6(4) . . ?
C15 C14 N17 122.3(4) . . ?
C13 C14 N17 120.1(4) . . ?
C16 C15 C14 119.6(5) . . ?
N11 C16 C15 123.0(4) . . ?
C19 N17 C14 124.2(4) . . ?
C19 N17 C18 117.2(4) . . ?
C14 N17 C18 118.1(4) . . ?
O20 C19 N17 120.4(4) . . ?
O20 C19 C31 119.8(4) . . ?
N17 C19 C31 119.8(4) . . ?
C26 N21 C22 116.7(4) . . ?
C26 N21 Ag 121.7(3) . . ?
C22 N21 Ag 121.6(3) . . ?
N21 C22 C23 123.4(4) . . ?
C22 C23 C24 119.4(4) . . ?
C25 C24 C23 117.7(4) . . ?
C25 C24 N27 122.5(4) . . ?
C23 C24 N27 119.7(4) . . ?
C26 C25 C24 119.1(4) . . ?
N21 C26 C25 123.6(4) . . ?
C29 N27 C24 125.5(4) . . ?
C29 N27 C28 117.4(4) . . ?
C24 N27 C28 117.0(4) . . ?
O30 C29 N27 120.8(4) . . ?
O30 C29 C33 119.3(4) . . ?
N27 C29 C33 119.9(4) . . ?
C32 C31 C36 119.3(4) . . ?
C32 C31 C19 117.8(4) . . ?
C36 C31 C19 122.6(4) . . ?
C31 C32 C33 121.0(4) . . ?
C32 C33 C34 119.4(5) . . ?
C32 C33 C29 117.6(4) . . ?
C34 C33 C29 122.6(4) . . ?
C35 C34 C33 119.5(5) . . ?
C36 C35 C34 121.0(4) . . ?
C35 C36 C31 119.6(5) . . ?
F41 B40 F43 103.4(11) . . ?
F41 B40 F44 108.3(16) . . ?
F43 B40 F44 108.9(11) . . ?
F41 B40 F42 110.2(13) . . ?
F43 B40 F42 113.4(11) . . ?
F44 B40 F42 112.2(11) . . ?
F53 B50 F52 108.4(10) . . ?
F53 B50 F54 107(2) . . ?
F52 B50 F54 110(2) . . ?
F53 B50 F51 111(2) . . ?
F52 B50 F51 111.3(18) . . ?
F54 B50 F51 108.9(10) . . ?
Cl73 C71 Cl72 111.4(8) . . ?
C71 Cl72 C71 89.8(10) . . ?
Cl73 Cl73 C71 113.6(5) . . ?
Cl82 C81 Cl83 115.6(8) . . ?
Cl92 C91 Cl93 128.1(15) . . ?
C91 Cl93 Cl93 154.0(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag N21 2.125(4) . ?
Ag N11 2.129(4) . ?
N11 C16 1.341(6) . ?
N11 C12 1.346(6) . ?
C12 C13 1.365(7) . ?
C13 C14 1.392(6) . ?
C14 C15 1.380(6) . ?
C14 N17 1.417(6) . ?
C15 C16 1.369(7) . ?
N17 C19 1.368(6) . ?
N17 C18 1.480(6) . ?
C19 O20 1.227(5) . ?
C19 C31 1.496(7) . ?
N21 C26 1.340(6) . ?
N21 C22 1.340(6) . ?
C22 C23 1.371(7) . ?
C23 C24 1.387(6) . ?
C24 C25 1.381(6) . ?
C24 N27 1.412(6) . ?
C25 C26 1.379(6) . ?
N27 C29 1.373(6) . ?
N27 C28 1.481(6) . ?
C29 O30 1.221(5) . ?
C29 C33 1.496(7) . ?
C31 C32 1.380(6) . ?
C31 C36 1.402(6) . ?
C32 C33 1.388(6) . ?
C33 C34 1.398(6) . ?
C33 C29 1.496(7) . ?
C34 C35 1.383(7) . ?
C35 C36 1.381(7) . ?
B40 F41 1.318(14) . ?
B40 F43 1.322(13) . ?
B40 F44 1.353(15) . ?
B40 F42 1.354(14) . ?
B50 F53 1.379(13) . ?
B50 F52 1.387(18) . ?
B50 F54 1.397(17) . ?
B50 F51 1.399(16) . ?
C71 Cl73 1.711(15) . ?
C71 Cl72 1.787(12) . ?
Cl72 C71 1.787(12) . ?
Cl73 Cl73 1.149(10) . ?
C81 Cl82 1.604(16) . ?
C81 Cl83 1.794(16) . ?
C91 Cl92 1.61(2) . ?
C91 Cl93 1.73(2) . ?
Cl93 Cl93 2.42(2) . ?
